Daylight-fluorescent textiles



Aug. 12, 1952 J. SWITZER EIAL DAYLIGHT-FLUORESCENT TEXTILES Filed Feb.13, 1942 INVENTORS JOSEPH L. SWITZER Mom/w A. WARD ATTORNEYS PatentedAug. 12, 1952 DAYLIGHT-FIUORESCENT TEXTILES 1 OFFICE 7 Joseph L.Switzer, Cleveland Heights, and

Richard A. Ward, Cleveland, Ohio Application February 13, 1942. SerialNo. 430,192 14 Claims. (01. 8 59) This invention relates to animprovement in fluorescent textiles and a method of dyeing textiles withfluorescent dyestuffs.

Brilliantly fluorescent fabrics have long been sought for theatricalcostumes and display purposes. Heretofore. even though the dyes employedwere brilliantly fluorescent, fluorescent dyed fabrics have been onlyweakly or faintly fluorescent and have been more or less characterizedby a certain muddiness or dullness of color, both under visible lightand invisible fiuorescigenous radiations, such as ultra-violet light.Consequently, when brilliantly fluorescent fabrics were requiredheretofore, suitable fabrics were varnished or coated with a coatingcontaining a dispersion of fluorescent dyes or pigments. Such coatedfabrics lost flexibility, porosity, and softness; garments made of suchcoated fabrics were uncomfortable and the coating tended to crack andbreak during use; such coated fabrics did not have a. satisfactory handand were difilcult to drape.

It is an object of this invention to provide a brilliantly fluorescentdyed fabric and. a process which will permit textiles, such as celluloseacetate, silk, wool, and the like, to be dyed with most knownfluorescent dyes to produce brilliantly fluorescent fabrics. Fluorescentfabrics dyed according to our method are particularly clean and pure incolor, both under visible light and invisible ultra-violet light and arenot appreciably affected by our dyeing process in respect toflexibility, porosity, softness, hand or drape. A further advantage ofour fluorescent dyed fabrics is that the natural shimmer and sheen oftextiles, such as satins, for example, is accentuated when dyed withfluorescent dyes by our method.

" A still further advantage of our invention is that fluorescent fabricsdyed by our method are not restricted to use in the somewhat narrowfield of theatrical costumes and displays. By

ourprocess it is possible to dye textileswith dyes claims and drawingsin which:

Fig. 1 is a greatly magnified diagrammatic cross-section of atextile'filament dyed according to the prior art methods; and

Fig. 2 is a greatly magnified diagrammatic cross-section of a textilefilament dyed according to our method.

As pointed out above, attempts to dye fabrics of the class describedwith a dyestuff which exhibited brilliant fluorescence in suitablesolutions heretofore generally produced a dyed fabric which was onlyweakly fluorescent and somewhat muddy in color. The same fabric dyedwith the same fluorescent dyestuffs by our method produce brilliantlyclear fluorescent dyed fabrics. While not restricting ourselves to anyone theory or reason for our success, we believe the contrast betweenthe results obtained by the use of our method and the methods of theprior art lies in the fact that in the prior art the problem of dyeingwas considered to be primarily one of selecting a suitable dyestuifwhch, under given conditions, would exhibit an amnity for the fibers orfilaments of a particular fabric-and, under such conditions, could beaflixed to such fibers or filaments more or less permanently in asubstantially and generally insoluble state. A filament of a textile sodyed is illustrated diagrammatically in Fig. 1.

In Fig. 1, l0 represents a filament of cellulose acetate and IIrepresents molecules of dye affixed to the filament at or onits surface.7 Where the dye molecules II are ones which exhibit color duetothephenomenon of absorption, 1. e., where a fractional band or bands ofwave lengths of the incident visible light are reflected and theremainder of the visible light is absorbed, such a concentration of dyeat the surface of the filament is satisfactory. Where the molecules Hare ones which exhibit color due to the phenomenon of fluorescence, i.e., where the dye molecules ll convert incident rays of fluorescigenousenergy, usually ultra-violet light, to

visible light of longer wave lengths, such a concentration of dye at thesurface of the filament -II is not satisfactory. Many fluorescentdyeemitted by some fluorescent dye particles may be largely absorbed byother dye particles.

As a result of our eiforts to analyze our fluorescent dyed fabrics andour method of dyeing, we believe that the problem of dyeing fabricsfluorescent is primarily one of avoiding a condition of concentration ofdye molecules on the surface of the fiber or filament to be dyed and,instead, obtaining a dispersion of the dye molecules in the fiber orfilament so that the dye molecules are probably oriented in the fiber orfilament in a relationship similar to the orientation of the dyemolecules when the dye is fluorescent in a solution. A filament of atextile so dyed is illustrated diagrammatically in Fig. 2. In

Fig. 2, represents a filament of cellulose acetate and 2! representsmolecules of a fluorescent dye dispersed in the filament by our processwhich will be described below. It is believed that thus neither incidentfiuorescigenous radiation nor emanated visible light will be lost due toan appreciable irreversible absorption of the radiations and the lightby the dye molecules. If the unexpectedly brilliant fluorescence offabrics dyed by our method is due to the orientation of the dyemolecules in or on the fibers similar to the orientation of the dyemolecules when in solution, we do not know why ourmethod of dyeingcauses such orientation of the dye, molecules.

Our method of dyeing a textile, cellulose ace- 0 tate satin, forexample, is, in general, as follows: A small quantity of a dyestuifwhich exhibits the desired fluorescent brightness in a suitable aqueousorganic solvent solution is dissolved in an aqueous solution of an ethylalcohol, for example. The percentage of dye in solution depends uponmany factors, such as the afiinity of the textile for the dye, thenecessary concentration of dye in the textile, and the like, but thepercentage of dye in solution is generally less than two percent. If agreater percentage of dye in solution is employed, it has been foundthat the fluorescent brightness of the dyed fabric is impaired. .Theaqueous alcoholic solution in which the dye is dissolved is preferably a40%, by weight, solution, but may vary from approximately to60%, byweight. Instead of ethyl alcohol we may, of course, use any similarsolvent or solvent mixture which is a mutual solvent for the dye andwater and which also exhibits a solvent or wetting action on the textileto be dyed. The dye is preferably one which exhibits less solubilityinwater than in the mutual solvent for the dye and water.

The cellulose acetate fabric is then dipped in the dye bath, preferablyby passing a festoon of the fabric through a vat of the dye bath, untilthe filaments of the fabric are dyed to the extent desired. Apparently,due to the wetting and penetrating properties of the ethyl alcohol aswell as its somewhat solvent and swelling action, the molecules of thedye are dispersed in the cellulose acetate filaments. The time thefabric remains in the dye bath, the temperature of the dye bath, theproportion of the ingredients in the dye bath, and the ratio of theweight ofthe dye to the weight of the fabric are all interrelatedfactors affecting the penetration and dispersion of the dye molecules inthe filaments of the textile and a change in any one will change theextent of penetration of the filaments by the dye. After the celluloseacetate fabric has been dipped in the dye bath, it is quickly flushedwith cold water to kill the dyeing action. All of the dyeing liquid onthe textile is thus washed off and the formation of dye crystals on thesurface of the fila- 4 ments is prevented. The fabric is then tentered,dried, and finished in the usual manner.

While the foregoing general description has dealt with the dyeing ofcellulose acetate, it is not to be understood that this method islimited to this specific textile. Other textiles may be advantageouslydyed by this process as will be apparent from the following specificexamples. While this invention is primarily concerned with the dyeing oftextiles, i. e., woven fabrics, it is to be understood that any fabricsor organic fibers or filaments, such as knitted fabrics, felts, yarns,

or loose flock may be dyed by this method. Further, it is to beunderstood that the following specific illustrations are given by way ofexample and are not to, be considered as being limitative eitherinrespect to the textiles named or the fluorescent dyes employed.

Example No. 1

One-tenth of one percent (0.1%) by weight of meta diethylaminophenolphthalein is dissolved in a 0%, by weight, solution of ethyl alcohol inwater to provide'a dye bath. To dry cellulose acetate fabric, asufiicient quantity of dye bath is employed so that the ratio of thefabric to the dye bath, by weight, will be approximately 15 parts ofcellulose acetate to 40 parts of the dye bath. With the dye bathmaintained at room temperature, the cellulose acetate fabric is immersedin the dye bath for 20 minutes and is then quickly and thoroughlyflushed with cool water to remove all traces of the dye bath. The fabricis then tentered and calendered in the usual manner. Cellulose acetatefabric so dyed fiuoresces a .brilliant red under ultra-violet light and,under visible white light, exhibits a brilliant fluorescent red colorbest suggested .by the name Neon Red.

Example No; 2

Two-tenths of one percent (0.2%) by weight of ethyl ester of metamonoethylaminophenol phthalein is dissolved in a 55%, by weight,solution of ethyl alcohol in water to provide a dye bath. To dye silkfabric, a suflicient quantity of dye bath is employed so that the ratioof the fabric to the dye bath, by weight, will be approximately 15 partsof silk to 60 parts of the dye bath. With the dye bath maintained atroom temperature, the silk fabric is immersed in the dye bath for 10minutes and is then quickly and thoroughly flushed with cool water toremove all traces of the dye bath. The fabric is then tentered andcalendered in the usual manner. Silk fabric so dyed fluoresces abrilliant salmon under ultra-violet light and exhibits a slightlyfluorescent red color under visible white light.

Example No. 3

Eight one-hundredths of one one percent (0.08%) by weight of p,p' di p"(p"' amincbenzolylamino benzoylamino stilbene 0,0 di (sodiumsulphonate)is dissolved in a 40%, by weight, solution of glycerine in water toprovide a dye bath. To dye cotton fabric, a sufficient. quantity of thedye bath is employed so that the ratio, by

Weight, will be approximately 15 parts of cotton stantially uncolored bythe dye, except for a slight blue jfluorescence under visible whitelight. I

i Example No. 4

Twelve one-hundredths of one percent (0.12 by weight offiminodi(p-dimethylaminophenol) methane hydrochloride is dissolved in a 35%,by weight, solution of acetone in water to provide a dye bath. To dyeWool fabric, a sufficient quantity of dye bath is employed so that theratio of the fabricto the dye bath will be approximately 15 parts ofwool to 90 parts of dye bath. With the dye bath maintained at 50 C., thewool fabric is immersed in the dye bath for 20 minutes and is thenquickly and thoroughly flushed with cool water toremove all traces ofthe dye bath. The fabric is then tentered andcalendered in the usualmanner. Wool fabric so dyed is brilliantly yellow-green underultra-violet light and exhibits a brightly fluorescent yellow colorunder visible white light.

' Example No. 5

One-tenth of one percent (0.1%) by weight of iminodi(p-dimethylaminophenol) methane hydrochloride is dissolved in a 35%,by weight, solution of isopropyl alcohol in water to provide a dye bath.To dye cellulose acetate fabric, a sufficient quantity of dye bath isemployed so that the ratio of the fabric to the dye bath will beapproximately 15 parts of fabric to 90 parts of dye bath. With the dyebath maintained at 50 C., the cellulose acetate fabric is immersed inthe dye bath for 15 minutes and is then thoroughly flushed with coolwater to remove all traces of the dye bath. The fabric is then tenteredand calendered in the usual manner. Cellulose acetate fabric so dyed isbrilliantly yellowgreen under ultra-violet light and exhibits a brightlyfluorescent yellow color under visible white light. 1

Example N056 One-tenth of one percent (0.1%) by weight, of metamethylethylaminophenol phthalein is dissolved in an aqueous solutioncontaining by weight, of ethylene glycol monomethylether and by Weight,of methyl alcohol to form a dye bath. To dye cellulose acetate fabric, asufficient quantity of dye bath is employed so that the ratio of thefabric to the'dye bath, by weight, will be approximately 15 parts ofcellulose acetate to 40 parts of dye bath. With the dye bath maintainedat 18 C., the cellulose acetate fabric is immersed in the dye bath for10 minutes and is then quickly and thoroughly flushed in cool water toremove all tracesvof the dye bath. The fabric is then tentered andcalendered in the usual manner. Cellulose acetate fabric so dyedfluoresces a brilliant red-orange under ultra-violet light and exhibitsa strong fluorescent red color under visible white light.

Example No. 7

Fifteen one-hundredths of one percent (0.15%), by weight, of metamonobutylaminophenol phthalein is dissolved in a 40%, by weight,solution of ethyl alcohol in water to form a dye bath. To dye celluloseacetate fabric, a sufficient quantity of dye bath is employed so thatthe ratio of the fabric to the dye bath, by weight, will beapproximately one part of cellulose acetate to two parts of dye bath.With the dye bath maintained at 20 C., the cellulose acetate fabric isimmersed in the dye bath or the dye bath is padded, on the celluloseacetate for 20 minutes and is then quickly and thoroughly flushed withcool"water to remove all traces of the dye bath. The fabric is thententered and calendered in the usual'manne'r. Cellulose acetate fabricso dyed fluoresces a bright'pastel' orange under ultraviolet light andexhibits a fluorescent pink color under visible white light.

From the foregoing, it is apparent that other daylight fluorescent dyesexhibiting a lesser solubility in water than in a mutual solvent for thedye and water may be employed to dye the same or other fabrics andtextiles, the proportionsof the dye, water and the mutual solvent in thedye bath, the time'the fabricremains in the dye bath and'the temperatureof the dye bath being determinable by experience in. each instance. 'Asa guide for thedetermination of such condition with respect toparticular daylight fluorescent dyes, the fabrics to be dyed, and thedaylight fluorescent shades to be obtained, it is to be noted that inthe following examples, the actual amount of dye held in a state akin tosolution in a given amount of fabric is probably very low, a factorwhich is insured by providing the dye baths with a relatively low amountof dye for the weight of fabric to be dyed thereby. Thus, in thepreceding examples, the'maxim-um possible concentrations of dyein'the'fabric (assuming complete exhaustion of the dye bath by thefabric, which is obviously not obtained by this solvent dyeing method)may be tabularized as follows:

Maximum Possible Example 1 part of fabric, in

percent) 9999999 ccmaaqmoom Q$QMHO While the actual percentage ofa givendaylight'fluorescent dye to be dispersed in a state akin to solution ina specific fabric of known composition, thickness, transparency, etc. toprovide a desired daylight fluorescent shade might be calculated, toobtain such calculated percentage of dye in cloth, it would involvefurther calculations of the absorption of a dissolved dye intothespecific fabric from the specific dye bath during given time andtemperature conditions. It is, therefore, more convenient and practicalto employ dye baths to fabric ratios in which the maximum possible dyein fabric ratios are in the order of those given above and then to shadethe fabric as desired without fear of over-dyeing, i. e., dischargingsuch a concentration of dye in the fabric that the dye cannot be held bythe'fabric in a non-daylight'fiuor'escent state in which the dye is notin a state akin to solution.

In the foregoing specification and the following claims, the termstrong, when applied to an aqueous solvent solution, denotes a solutionin which the percentage of non-aqueous solvent or solvent mixture rangesfrom approximately 25% to 60%, by weight, of the aqueous solventsolution; when such strong aqueous solvent solutions are employed in adye bath for cellulose acetate fabric, the percentage of non-aqueoussolvent, by weight, preferably ranges from approximately 35% to 40% and,by keeping the temperatures of the solvent solutions in contact with thecellulose acetate,-during both dyeing and flushing,

down to thepoint where the intense swelling action of the solution; onthe fabric cannot proceed beyond-incipient coalescence, the rapiddilution of 'th'e sblution during "flushing will allow the filaments ofthe fabric to return to their unswollen condition and prevent alterationof the hand of the fabric. The term cool, when applied tothe water forflushing the dye bath from the fabric, isintended to denote water havinga temperature less than approximately 100 F.; preferably'water havingthe temperature of ordinary tapwater, i; e., from 55 to 75 F., isusually employed; The term daylight fluorescen is employed to denote thephenomenon exhibited by materials-which not only reflect portions of thespectrum of incident visible light but simultaneously fluoresce underthe influence of the incident light. It is apparent therefore, that thisinvention is not, limited to the particular examples disclosed, but bythe following claims.

What is claimed is: r

l. The process of dyeing to produce a daylight fluorescent fabriccomprisingthe steps of providing a dye bath by dissolving a daylightfluorescent dye in a strong aqueous alcoholic solution, said dye beingcharacterized by a greater solubility in alcohol than in water,immersing in the dye bath a fabric, characterized by its tendency to beswollen bythe aqueous alcoholic solution and to absorb said dye in astate akin to solution, maintaining the temperature of said dye bathbelow that which swells the filaments of said fabric to coalescence, andthen flushing the fabric with cool water to remove said dye bath.

2. The method of dyeing a fabric as defined in claim 1 in which thealcohol in the aqueous alcoholic solution is substantially forty percentby weight.

3. The method of dyeing cellulose acetate fabric comprising the steps ofproviding a dye bath by dissolving a daylight fluorescent dye in astrong solution of a solvent and water, said dye being characterized byits lesser solubility in water than in said solvent in which solventsaid dye, water and cellulose acetate are each soluble, immersing. insaid dye bath cellulose acetate fabric characterized by its tendency tobe swollen to incipient coalescence by said dye bath, removing saidfabric before coalescence, and then flushing-said cellulose acetate withwater to remove said dye bath.

, 4. The method of dyeing cellulose acetate fabric comprising the stepsof dissolving a daylight fluorescent dye, characterized by a greatersolubility in alcohol than in Water, in a strong solution of alcohol inwater to form a dye bath, immersing cellulose acetate fabric in said dyebath, said dye bath and said fabric being proportioned so that themaximum possible absorption of dye into said fabric cannot exceed 0.8%,by weight, of the fabric, maintaining said dye bath below thattemperature at which said dye bath swells the filaments of the fabric tocoalescence, and flushing said cellulose acetate fabric with cool waterto-remove said dye bath.

5. The method, of dyeing cellulose acetate fabric to provide a daylightfluorescent fabric comprising the steps of providing a dye bath bydissolving a fluorescent dye derived from dialkylaminophenol in a strongaqueous solution of alcohol, said dye being less than two per cent, by

weight, of said a solution, immersing cellulose acetate fabric in saiddye bath, maintaining said dye-bath below the temperature at which thedye bath causes thefllaments of the fabric to coalesce,

8 and then flushing said cellulose acetate fabric with cool water toremove said dye bath.

6. The method of dyeing cellulose acetate fabric to provide a daylightfluorescent fabric comprising the steps of providing a dye bath bydissolving a fluorescent dye derived from monoalkylaminophenol in astrong aqueous solution of alcohol, said dye being less than two percent, by weight, Of said solution, immersing cellulose acetate fabric insaid dye bath, maintaining said dye bath below the temperature at whichthe dye bath causes thefilaments of the fabric to coalesce, and thenflushing said cellulose acetate fabric with cool water to remove saiddye bath.

7. The method of dyeing cellulose acetate fabric to provide a daylightfluorescent fabric comprising the steps of providing a dye bath bydissolving a fluorescent dye derived from diethylaminophenol in a strongaqueous solution of alcohol, said dye being less than two per cent, byweight, of said solution, immersing cellulose acetate fabric in said dyebath, maintaining said dye bath below the temperature at which the dyebath causes the filaments of the fabric to coalesce, and then flushingsaid cellulose acetate fabric with cool water to remove said dye bath.

8. As a composition of matter, a dyed fabric comprising a fabric oforganic filaments and a daylight fluorescent dye dispersed in saidfilaments of said fabric, said dye exhibiting a lesser solubility inwater than in an organic solvent for said dye and water, said dye beingso 'arranged and oriented in said filaments of said fabric that saidfabric exhibits daylight fluorescence.

9. As a composition of matter, a dyed fabric comprising a fabric ofcellulose acetate filaments and a daylight fluorescent dye dispersed insaid filaments, said dye exhibiting a lesser solubility in Water than inan organic solvent for said dye and water, said dye being so arrangedand oriented in said filaments of said fabric that said fabric exhibitsdaylight fluorescence.

10. As .a composition of matter, a dyed fabric comprising a fabric ofcellulose acetate filaments and a fluorescent dye derived frommonoalkylaminophenol so dispersed and oriented in said filaments thatsaid fabric exhibits daylight fluorescenoe.

11. As a composition of matter, a dyed fabric comprising a fabric ofcellulose acetate filaments and a fluorescent dye derived fromdialkylaminophenol so dispersed and oriented in said filaments that saidfabric exhibits daylight fluorescence.

12..As a composition of matter, a dyed fabric comprising a fabric ofcellulose acetate filaments and afiuorescent dye derived fromdiethylaminophenol so dispersed and oriented in said filaments that saidfabric exhibits daylight fluorescence.

13. The process of dyeing to produce a daylight fluorescent fabriccomprising the steps of providing an aqueous dye bath containing notmore than two per cent, by Weight, of a daylight fluorescent dye insolution, immersing in said dye bath a fabric characterized by itstendency to absorb said dye in a state akin to solution and to beswelled by the dye bath, the Weight of fabric immersed in said bathbeing proportioned to the weight of dye in said bath so that the maximumpossible weight of dye which can be absorbed into said fabric will notexceed 0.8% of the weight of the fabric, maintaining said fabric in saiddye bath until the dye has penetrated into the fabric in a state akin tosolution, maintaining the temperature of the dye bath below that atwhich 9 said dye bath swells the filaments of said fabric tocoalescence, and then flushing the fabric to remove said dye bath.

14. The process of dyeing to produce a daylight fluorescent fabriccomprising the steps of providing a dye bath by dissolving a daylightfluorescent dye in a strong aqueous solution of a mutual solvent forsaid dye and water, said solvent also constituting a swelling agent forthe fabric to be dyed, immersing in said dye bath a fabric characterizedby its tendency to absorb said dye in a state akin to solution, theweight of fabric immersed in said dye bath being proportioned withrespect to the weight of said dye bath so that the maximum possibleweight of dye which can be absorbed by said fabric will not exceed 0.8%of the weight of said fabric, maintaining said fabric in said dye bathuntil said dye is absorbed into the filaments of said fabric in a stateakin to solution, maintaining the temperature of said dye bath below thetemperature causing incipient coalescence during the time said dye isbeing absorbed, removing said fabric from said dye bath and thenflushing the fabric in cool water to remove said dye bath.

JOSEPH L. SWITZER. RICHARD A. WARD.

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John

Synthetic Dyestuffs, 6th

8. AS A COMPOSITION OF MATTER, A DYED FABRIC COMPRISING A FABRIC OFORANIC FILAMENTS AND A DAYLIGHT FLUORESCENT DYE DISPERSED IN SAIDFILAMENTS OF SAID FABRIC, SAID DYE EXHIBITING A LESSER SOLUBILITY INWATER THAN IN AN ORGANIC SOLVENT FOR SAID DYE AND WATER, SAID DYE BEINGSO ARRANGED AND ORIENTED IN SAID FILAMENTS OF SAID FABRIC THAT SAIDFABRIC EXHIBITS DAYLIGHT FLUORESCENCE.